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Treatment method for methyltestosterone mother liquor

A treatment method, the technology of methyltestosterone, applied in the field of chemical pharmaceuticals, can solve problems such as ecological environmental hazards, resource waste, and environmental pollution, and achieve the effects of reducing production costs, reducing pollution, and avoiding waste

Inactive Publication Date: 2017-04-26
HUAZHONG PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] (3) It is extremely difficult to recover methyltestosterone from the mother liquor by recrystallization, and it is impossible to obtain a product that meets the quality requirements after repeated recrystallization
[0009] Methyltestosterone mother liquor is difficult to deal with. Usually, the mother liquor is discharged into the environment after simple treatment, which not only causes waste of resources and pollutes the environment, but also because the hormone substances contained in the mother liquor will bring great harm to the ecological environment.
At present, there are no public reports at home and abroad on the recovery and treatment process for the mother liquor of methyltestosterone

Method used

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  • Treatment method for methyltestosterone mother liquor

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Take 100ml methyltestosterone mother liquor, add ethyl acetate and continue to concentrate under reduced pressure until viscous. Then add 40ml of ethyl acetate and 60ml of petroleum ether and stir to dissolve, continue to add 50ml of acetone cyanohydrin and 16ml of diethylamine, and heat up at 40°C to 45°C for 28 hours. Concentrate under reduced pressure to viscous, freeze and cool down to below 5°C, filter and dry to obtain 65.8g of intermediate materials;

[0026] Add 65.8g of the intermediate material obtained in the previous step into 350ml of methanol, stir evenly, add dropwise a solution of 16g ​​of potassium hydroxide dissolved in 50ml of water at 25°C to 30°C, heat up at 50°C to 55°C and keep it warm for reaction 3 Hour. After filtering, add an aqueous solution of acetic acid dropwise to the filtrate to neutralize to pH 6-7. Concentrate under reduced pressure to a paste, add water for water analysis, filter, wash with water, and dry to obtain the crude 4-andro...

Embodiment 2

[0028] Take 100ml methyltestosterone mother liquor, add ethyl acetate and continue to concentrate under reduced pressure until viscous. Then add 100ml of ethyl acetate and 100ml of petroleum ether and stir to dissolve, continue to add 44ml of acetone cyanohydrin and 8ml of triethylamine, and heat up at 35°C to 40°C for 25 hours. Concentrate under reduced pressure to viscous, freeze and cool down to below 5°C, filter and dry to obtain 68.3g of intermediate materials;

[0029] Add 68.3g of the intermediate material obtained in the previous step into 350ml of methanol, stir evenly, add dropwise a solution of 20g of sodium hydroxide dissolved in 60ml of water at 25°C to 30°C, and heat up at 50°C to 55°C for 3.5 Hour. After filtering, add an aqueous solution of acetic acid dropwise to the filtrate to neutralize to pH 6-7. Concentrate under reduced pressure to a paste, add water for water analysis, filter, wash with water, and dry to obtain the crude 4-androstenedione. Add the cru...

Embodiment 3

[0031] Take 100ml methyltestosterone mother liquor, add ethyl acetate and continue to concentrate under reduced pressure until viscous. Then add 100ml of ethyl acetate and 200ml of petroleum ether and stir to dissolve, continue to add 48ml of acetone cyanohydrin and 9ml of triethylamine, and heat up at 35°C to 40°C for 24 hours. Concentrate under reduced pressure to viscous, freeze and cool down to below 5°C, filter and dry to obtain 67.5g of intermediate materials;

[0032] Add 67.5g of the intermediate material obtained in the previous step into 350ml of methanol, stir evenly, add dropwise a solution of 18g of sodium hydroxide dissolved in 50ml of water at 25°C to 30°C, heat up at 50°C to 55°C and keep it warm for reaction 4 Hour. After filtering, add an aqueous solution of acetic acid dropwise to the filtrate to neutralize to pH 6-7. Concentrate under reduced pressure to a paste, add water for water analysis, filter, wash with water, and dry to obtain the crude 4-androste...

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Abstract

The invention discloses a treatment method for methyltestosterone mother liquor. The treatment method comprises the following steps that 1, an ethyl acetate evaporation solvent is added into the methyltestosterone mother liquor, then, a mixed solvent, acetone cyanohydrin and organic aliphatic amine are added for reacting, and an intermediate material is obtained; 2, methyl alcohol is added into the intermediate material obtained in the first step, after uniform stirring, alkaline water is added for reacting, and crude 4-androstenedione is obtained; crude 4-androstenedione is refined, and refined 4-androstenedione is obtained through concentration, freezing and filtering; filter liquor obtained through filtering in the refining process of refined 4-androstenedione is subjected to concentration, freezing, filtering and recrystallization, and methyltestosterone is obtained. By means of the method, emissions of hormone waste are reduced, and pollution to the environment is reduced; 4-androstenedione and methyltestosterone can be recycled, recycled 4-androstenedione can be utilized again for methyltestosterone production, resource waste is avoided, and the production cost is greatly reduced.

Description

technical field [0001] The invention belongs to the field of chemical pharmacy, and in particular relates to a method for treating methyltestosterone mother liquor. Background technique [0002] The structural formula of methyltestosterone (17α-methyl-17β-hydroxyandrost-4en-3one) is: [0003] [0004] Methyltestosterone, as an androgen drug, is clinically applicable to promoting the development of male sexual organs and secondary sexual characteristics and maintaining their normal functions; female functional uterine bleeding and migratory breast cancer, etc. The steroid compound is also an important intermediate for the preparation of various drugs such as Mandrosterone, 4-Chloromethorone, Fluoxymesterone, and 4-Hydroxymethyltestosterone, and is widely used in the market. Methyltestosterone is obtained from 4-androstenedione (4-androstene-3,17-dione) as raw material, followed by 3-keto protection, 17-keto Grignard addition, and hydrolysis. The crude product was recryst...

Claims

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Application Information

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IPC IPC(8): C07J1/00
CPCC07J1/0037
Inventor 廖俊刘玉亭付林曾建华徐明琴李桂莲田玉林
Owner HUAZHONG PHARMA
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